HAP solids were prepared with different Ca/P ratios and Na+ cations before being characterized by XRD, XPS, LEIS, NMR, IR, and TGA. Their acid–base properties were then measured and discussed in relation to the characterization results.
The Guerbet reaction of ethanol to produce heavier products was performed over a series of extensively characterized carbonate-containing hydroxyapatites (HAPs) with different Ca/P ratios and thus different densities, strengths and natures of acid and basic sites. These properties were correlated with the reactivity of the solids and an optimal ratio between the amount of acid and basic sites was evidenced (ca. 5). The best performance was accordingly obtained over the Hap-CO 3 catalyst, which gave a yield of 30% of heavier alcohols at 40% ethanol conversion.Catal. Sci. Technol. This journal is † Electronic supplementary information (ESI) available: Supplementary correlations drawn between isopropanol and ethanol reactivity and supplementary correlations drawn between directly measured acid-base properties and ethanol reactivity. See
The Guerbet reaction of ethanol to heavier products was performed over a series of extensively characterized Sr‐substituted hydroxyapatites (HAPs) with different (Ca+Sr)/P ratios, and thus different structural, textural, and acid–base properties. The acid–base properties were correlated with the reactivity of the solids and an optimal ratio between the amount of acid and basic sites was determined (ca. 4), whereas the ethanol conversion was mainly depending on the specific surface area of the solids. The stoichiometric 100 mol % Sr‐substituted sample (SrAp‐100) was especially efficient in higher alcohols production, which can be illustrated by a total alcohol selectivity (76.4 %) higher than that of all the other solids at a 13 % ethanol isoconversion.
High-throughput (HT) methodology was applied for the synthesis, characterization and catalytic testing of Cu-and Ni-based catalysts for glucose hydrogenation. Design of Experiment (DoE) was used in all steps. The deposition and reduction of both metals was performed using chemical reduction with hydrazine method. In total 36 catalysts were synthetized, characterized and tested in 5 days. The amount of metal deposited on the support was chosen as the discriminative and determining parameter. The catalysts were tested at low temperature in the hydrogenation of glucose to sorbitol. The results showed that chemical reduction-precipitation method could be performed using fully automatized robots. The deposition of the metals strongly depended on the nature of the support, the temperature of the reduction and hydrazine/H2O ratio. The maximum metal precipitation occurred at higher temperature (70°C) and lower N2H4/H2O ratio (0.04 mol/mol) in both cases. The results clearly showed that glucose conversion is higher for the catalysts synthesized at 70°C compared to the catalysts synthesized at 50°C, irrespective of the metal precursors, supports and hydrazine/water ratios employed during catalysts syntheses. With a total timespan of around 5 days we showed that HT methods applied to all the steps (synthesis, characterization and testing) can significantly reduce the time needed to develop a new catalytic process.
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